Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of sym-trifluorobenzene

A technology of trifluorobenzene and mes-trichlorobenzene, applied in the field of preparation of mes-trifluorobenzene, can solve problems such as being unsuitable for large-scale industrial production, cumbersome synthesis route, difficult and low-cost, etc., and achieves easy operation, easy separation and recovery, solvent The effect of less denaturation

Active Publication Date: 2017-09-08
DALIAN QIKAI MEDICAL TECH
View PDF8 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Numerous patents and journals at home and abroad have reported the preparation methods of fluorine-containing aromatic compounds without strong charge-absorbing groups, such as s-trifluorobenzene, but these methods are either energy-intensive, difficult to implement at low cost, or synthesized The route is cumbersome and unreasonable, only suitable for laboratory-scale research work and not suitable for large-scale industrial production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 134g of potassium fluoride, 350ml of benzonitrile and 300ml of toluene in sequence into a 1000ml four-necked flask equipped with a water separator. Heat to reflux at 120-130°C under mechanical stirring, separate water, turn on the water separator switch and heat to 185°C to remove toluene after no water is separated. After no toluene evaporated, the temperature was lowered to room temperature under nitrogen protection and transferred to a 1000ml autoclave, and 250g of 3,5-difluorochlorobenzene, 17g of tetraphenylphosphonium bromide and 5g of nitrobenzene were added, and the temperature was raised to 240°C for 30 hours. After the reaction is finished, the reaction system is distilled under normal pressure and the fraction at 40-160° C. is received. A 30cm packed rectification column is used to carry out atmospheric rectification on the above receiver, and simultaneously receive the 67-69°C fraction to obtain a final product with a purity of more than 99%, with a yiel...

Embodiment 2

[0030] Add 134g of potassium fluoride, 350ml of benzonitrile and 300ml of toluene in sequence into a 1000ml four-necked flask equipped with a water separator. Heat to reflux at 120-130°C under mechanical stirring, separate water, turn on the water separator switch and heat to 185°C to remove toluene after no water is separated. After no toluene is evaporated, nitrogen protection is used to cool down to room temperature and transfer to a 1000ml autoclave, and 100g of trichlorobenzene, 17g of tetraphenylphosphonium bromide and 5g of nitrobenzene are added, and the temperature is raised to 190°C for 10 hours. / min to 240°C and hold for 25 hours. After the reaction is finished, the reaction system is distilled under normal pressure and the fraction at 40-160° C. is received. A 30cm packed rectification column is used to carry out atmospheric rectification on the above receiver, and simultaneously receive the fraction at 67-69°C to obtain a final product with a purity of more than...

Embodiment 3

[0032] Add 134g of potassium fluoride, 350ml of benzonitrile and 300ml of toluene in sequence into a 1000ml four-necked flask equipped with a water separator. Heat to reflux at 120-130°C under mechanical stirring, separate water, turn on the water separator switch and heat to 185°C to remove toluene after no water is separated. After no toluene is evaporated, cool down to room temperature under nitrogen protection and transfer to a 1000ml autoclave, add 250g 3,5-difluorochlorobenzene, 15g tetrakis(diethylamino)phosphonium bromide and 5g nitrobenzene, and heat up to 240°C React for 30 hours. After the reaction is finished, the reaction system is distilled under normal pressure and the fraction at 40-160° C. is received. A 30cm packed rectification column is used to carry out atmospheric rectification on the above receiver, and simultaneously receive the 67-69°C fraction to obtain a final product with a purity of more than 99%, with a yield of 70.1%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method of sym-trifluorobenzene and belongs to the field of chemical production processes. The preparation method of sym-trifluorobenzene is characterized by comprising the following steps: (1) mixing potassium fluoride with an aprotic polar solvent to obtain a mixed liquid; (2) adding a reaction primer, nitrobenzene and a phase transfer catalyst into the mixed liquid, wherein the reaction primer is sym-trichlorobenzene or 3,5-difluorobenzene to obtain a reaction system; (3) putting the reaction system obtained in the step (2) into a high pressure kettle, removing air in the kettle and sealing the kettle, and reacting to obtain a product; and (4) rectifying the product which is distilled to obtain the sym-trifluorobenzene. The method provided by the invention is relatively low in energy consumption, few in side reaction, simple in reaction step and easy to operate. The denaturation amount of a solvent is small, and the solvent is easily separated and recovered. Compared with other methods, the preparation method is greener and more environment-friendly.

Description

technical field [0001] The invention relates to a preparation method of s-trifluorobenzene, which belongs to the field of chemical production technology. Background technique [0002] Trifluorobenzene is usually a colorless transparent liquid and is an important basic chemical raw material. It has broad application prospects in chemical engineering, pharmaceutical liquid crystal materials, etc. [0003] Trifluorobenzene is a typical fluorine-containing aromatic compound, and there are many methods for its synthesis, among which Balz-Schiemann, HF-diazotization and halogen exchange methods have been relatively perfect. However, the first two methods must go through the process of diazotization and then fluorination, both of which require the use of toxic reagents, are also relatively dangerous, and have a long route and high cost, so they have been gradually eliminated in industry. Although the synthesis of fluorine-containing aromatic compounds by halogen exchange fluorinat...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C17/20C07C17/383C07C25/13
Inventor 田瀚卿姜殿平张洪学张忠
Owner DALIAN QIKAI MEDICAL TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com